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熒光碳量子點(diǎn)的合成、性能及分析檢測(cè)應(yīng)用研究

發(fā)布時(shí)間:2018-06-18 00:51

  本文選題:碳量子點(diǎn) + 水熱法; 參考:《寧夏大學(xué)》2017年碩士論文


【摘要】:碳量子點(diǎn)(簡(jiǎn)稱碳點(diǎn))作為一種新型的零維碳納米材料,具有粒徑小、毒性低、生物相容性好、激發(fā)光連續(xù),發(fā)射光可調(diào)等優(yōu)點(diǎn)。與傳統(tǒng)熒光材料相比,碳量子點(diǎn)具有更為突出的光學(xué)特性及優(yōu)越的性能,所以其在生物成像、光電器件、催化、生物傳感等領(lǐng)域都表現(xiàn)出十分重要的應(yīng)用價(jià)值。本論文采用不同的碳源,通過(guò)水熱法輔助硝酸氧化法制備出了性能優(yōu)良碳量子點(diǎn),并且對(duì)合成的熒光碳點(diǎn)進(jìn)行元素?fù)诫s以提高碳量子點(diǎn)的熒光性能。利用合成的熒光碳量子點(diǎn)構(gòu)建了檢測(cè)的過(guò)氧化氫、Fe2+、Fe3+、L-半胱氨酸、Hg2+以及有機(jī)磷農(nóng)藥的光學(xué)傳感方法。具體研究?jī)?nèi)容如下:1、以玉米秸稈為碳源,采用一步水熱法合成了發(fā)藍(lán)綠色熒光的碳量子點(diǎn)(CDs),并對(duì)合成的碳量子點(diǎn)進(jìn)行了 TEM、XRD、XPS、FTIR等表征,證實(shí)了合成的CDs表面被羧基、羥基、氨基、羰基等官能團(tuán)所功能化;熒光碳量子點(diǎn)粒徑在5.2nm左右并且具有良好的分散性和水溶性,量子點(diǎn)產(chǎn)率達(dá)到了 7.6%。研究發(fā)現(xiàn)過(guò)氧化氫和Fe2+同時(shí)存在的條件下,CDs的熒光會(huì)發(fā)生猝滅,基于此原理實(shí)現(xiàn)了對(duì)過(guò)氧化氫和Fe2+靈敏的檢測(cè),最低檢測(cè)線為0.18 μmnol/L和0.21 μmol/L。2、采用太西煤為碳源,通過(guò)硝酸氧化法及水熱輔助合成了發(fā)黃色熒光的石墨烯量子點(diǎn)(GQDs),實(shí)驗(yàn)中對(duì)比了硝酸氧化法制備的GQDs與水熱輔助合成的GQDs的熒光性能,通過(guò)對(duì)兩種方法合成的GQDs進(jìn)行了 TEM、XPS、FTIR、UV-vis等表征,對(duì)比分析了 GQDs的結(jié)構(gòu)性能,合成的GQDs的粒徑在4.5 nm左右;贔e3+可以使GQDs的熒光發(fā)生猝滅的原理,實(shí)現(xiàn)了靈敏的檢測(cè)Fe3+,在PBS緩沖溶液中(0.02mol/LpH=3.02),GQDs的熒光強(qiáng)度與Fe3+的濃度在0-21 μmol/L范圍內(nèi)呈良好的線性關(guān)系,最低檢測(cè)線為0.67nmol/L,并將本方法應(yīng)用到對(duì)水樣中Fe3+的檢測(cè)。3、以海藻酸為碳源,氫氧化鎂和三乙醇胺為修飾試劑,通過(guò)一步水熱法合成了水溶性好且穩(wěn)定性高的鎂氮共摻雜的碳量子點(diǎn)(Mg,N-CDs)。研究發(fā)現(xiàn)Hg2+對(duì)碳量子點(diǎn)熒光強(qiáng)度有良好的猝滅作用,當(dāng)加入L-半胱氨酸時(shí),碳量子點(diǎn)的熒光強(qiáng)度又會(huì)恢復(fù),基于熒光開(kāi)關(guān)的原理,可以快速、靈敏且選擇性好的檢測(cè)Hg2+和L-半胱氨酸。實(shí)驗(yàn)結(jié)果表明:在pH=7的磷酸鹽緩沖溶液中碳量子點(diǎn)的熒光強(qiáng)度與Hg2+濃度在0-45 μmol/L范圍內(nèi)呈良好的線性關(guān)系,最低檢測(cè)限為0.17 μmol/L。L-半胱氨酸的檢測(cè)范圍在0-55 mol/L,最低檢測(cè)限為0.09 μmol/L。4、鎂氮共摻雜的碳量子點(diǎn)可以作為一種熒光探針高靈敏度和選擇性的檢測(cè)有機(jī)磷農(nóng)藥的中的對(duì)氧磷。當(dāng)體系中分別加入解磷定(PAM)和有機(jī)磷農(nóng)藥(OPs)時(shí),Mg,N-CDs的熒光強(qiáng)度基本上沒(méi)有發(fā)生變化,當(dāng)同時(shí)加入PAM和OPs時(shí),碳量子點(diǎn)的熒光強(qiáng)度會(huì)明顯的猝滅。本章還考察了檢測(cè)條件如:pH、反應(yīng)時(shí)間,PAM的濃度對(duì)檢測(cè)有機(jī)磷的影響。在最佳檢測(cè)條件下,有機(jī)磷的檢測(cè)范圍為0.05-45 μmol/L,最低檢測(cè)限為0.87 μmol/L。
[Abstract]:Carbon quantum dots (carbon dots), as a new kind of zero-dimensional carbon nanomaterials, have the advantages of small particle size, low toxicity, good biocompatibility, continuous excitation light and adjustable emission light. Compared with traditional fluorescent materials, carbon quantum dots (QDs) have more outstanding optical properties and superior properties, so they have important application value in biological imaging, optoelectronic devices, catalysis, biosensor and so on. In this paper, carbon quantum dots with excellent properties were prepared by hydrothermal assisted nitric acid oxidation with different carbon sources, and the synthesized carbon dots were doped with elements to improve the fluorescence properties of carbon quantum dots. An optical sensing method for the determination of Fe _ 2H _ 2O _ 2, Fe _ 3, L-cysteine, Hg2 and organophosphorus pesticides was constructed by using the synthesized fluorescent carbon quantum dots (FQDs). The specific research contents are as follows: 1. Using corn straw as carbon source, a blue-green fluorescent carbon quantum dot (CDsN) was synthesized by a one-step hydrothermal method. The synthesized QDs were characterized by TEMN XRDX PSN FTIR and the surface of the synthesized CDs was confirmed by carboxyl group, hydroxyl group, amino group, etc. The particle size of fluorescent carbon quantum dots is about 5.2nm and has good dispersion and water solubility. The yield of quantum dots reaches 7.6. It was found that the fluorescence of CDs would be quenched under the condition of both hydrogen peroxide and Fe _ 2. Based on this principle, the sensitive detection of hydrogen peroxide and Fe _ 2 was realized. The lowest detection line was 0.18 渭 mol / L and 0.21 渭 mol / L ~ (-2), and the coal was used as carbon source. GQDs with yellow fluorescence were synthesized by nitric acid oxidation and hydrothermal assisted synthesis. The fluorescence properties of GQDs prepared by nitric acid oxidation and hydrothermal assisted synthesis were compared. The GQDs synthesized by the two methods were characterized by the UV-vis method. The structure and properties of the synthesized GQDs were compared and analyzed. The size of the synthesized GQDs was about 4.5 nm. Based on the principle that Fe _ 3 can quench the fluorescence of GQDs, a sensitive method for the detection of Fe _ 3 has been achieved. The fluorescence intensity of GQDs in PBS buffer solution is in good linear relationship with the concentration of Fe _ 3 in the range of 0-21 渭 mol 路L ~ (-1), and the fluorescence intensity of GQDs is 0.02mol / L ~ 3.02mol / L in PBS buffer solution. The lowest detection line was 0.67 nmol / L, and the method was applied to the determination of Fe _ 3 in water samples by using alginic acid as carbon source, magnesium hydroxide and triethanolamine as modifiers. Mg-N doped carbon quantum dots (MQDs) with good water solubility and high stability were synthesized by one step hydrothermal method. It is found that Hg _ 2 has a good quenching effect on the fluorescence intensity of carbon quantum dots. When L- cysteine is added, the fluorescence intensity of carbon quantum dots will recover again. Based on the principle of fluorescence switch, the fluorescence intensity of carbon quantum dots can be recovered quickly. Sensitive and selective detection of Hg 2 and L-cysteine. The experimental results show that the fluorescence intensity of carbon quantum dots in phosphate buffer solution at pH 7 has a good linear relationship with the concentration of Hg _ 2 in the range of 0-45 渭 mol / L. The lowest detection limit is 0.17 渭 mol / L L- cysteine in the range of 0-55 mol / L, and the lowest detection limit is 0.09 渭 mol / L. 4. The magnesia-nitrogen co-doped carbon quantum dots can be used as a fluorescent probe to detect p-oxyphosphorus in organophosphorus pesticides with high sensitivity and selectivity. The fluorescence intensity of MgN-CDs was basically unchanged when PAM) and OPs were added respectively. When PAM and ops were added at the same time, the fluorescence intensity of carbon quantum dots was obviously quenched. The influence of the concentration of PAM on the determination of organophosphorus was also investigated. Under the optimum conditions, the detection range of organophosphorus was 0.05-45 渭 mol / L, and the minimum detection limit was 0.87 渭 mol / L.
【學(xué)位授予單位】:寧夏大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:O657.3;TB383.1

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